CN104377369A - Fibrous electrochemical light-emitting battery and a preparing method thereof - Google Patents
Fibrous electrochemical light-emitting battery and a preparing method thereof Download PDFInfo
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- CN104377369A CN104377369A CN201410555186.7A CN201410555186A CN104377369A CN 104377369 A CN104377369 A CN 104377369A CN 201410555186 A CN201410555186 A CN 201410555186A CN 104377369 A CN104377369 A CN 104377369A
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- fibrous
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/36—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the electrodes
- H01L33/40—Materials therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
- H01M4/08—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/04—Cells with aqueous electrolyte
- H01M6/06—Dry cells, i.e. cells wherein the electrolyte is rendered non-fluid
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0016—Processes relating to electrodes
Abstract
The invention belongs to the technical field of electrochemical light-emitting batteries, and specifically to a fibrous electrochemical light-emitting battery and a preparing method thereof. According to the battery, a metal wire is used as a fiber substrate electrode, and a method of coaxially winding a multi-wall orientated carbon nanotube film is adopted, so that the multi-wall orientation carbon nanotube film can be wrapped on a fibrous electrochemical light-emitting battery body and can be used as an outer layer transparent electrode; a light emitting polymer is sandwiched between two electrodes to form the fibrous light-emitting electrochemical battery. The multi-wall orientated carbon nanotube film has the good light transmittance and conductivity, is a good transparent electrode material, so that the luminous efficiency of the fibrous light-emitting electrochemical battery is greatly improved, and the cost is greatly reduced.
Description
Technical field
The invention belongs to electrochemical luminescence cell art, concrete one relates to fibrous electrochemical luminescence battery and preparation method thereof.
Background technology
Since Japanese Iijima Late Cambrian carbon nano-tube in 1991, carbon nano-tube is subject to people with performances such as the mechanics of its uniqueness, electricity, calorifics and payes attention to widely, has good development prospect, will become active material of new generation.
Carbon nano-tube can be divided into Single Walled Carbon Nanotube and multi-walled carbon nano-tubes according to the number of graphite flake layer.Unique carbon nano tube structure imparts mechanics, the electric property of its excellence, if Young's modulus is up to 1000 lucky handkerchiefs (being about 5 times of steel), hot strength is up to 63 lucky handkerchiefs (being about 50 times of steel). and due to the physical property of lower density (being about 1/6 of steel), higher intensity, higher conductivity and other excellences of carbon nano-tube, carbon nano-tube is considered to there is huge application prospect at wide spectrums such as structural material, electronic device, Flied emission, biological medicine and electrochemistry.Meanwhile, carbon nano-tube is widely used in the fields such as luminescent device, polymer solar battery and ultracapacitor.
Along with the development need of hyundai electronics cause, luminescent device becomes more and more important.As adopted the Organic Light Emitting Diode and electrochemical luminescence battery etc. of flexible substrates, formation can luminescent device [1-20,24].But these luminescent devices can not meet lightweight, the small and exquisite and demand for development that can weave.
Following demand for development is that microdevice has luminescence or Presentation Function, does not still have bibliographical information threadiness electrochemical luminescence battery at present.The main difficulty making fibrous electrochemical luminescence battery is its good interracial contact, and finds suitable transparent flexible electrode.If can solve the problem, fibrous electrochemical luminescence battery can have extraordinary prospect in the development in future.In the near future, fibrous electrochemical luminescence battery will be had very important significance.
Summary of the invention
The object of the present invention is to provide fibrous electrochemical luminescence battery that a kind of luminous efficiency is high, cost is low and preparation method thereof.
Fibrous electrochemical luminescence battery provided by the invention, comprising: a wire, and as fibrous substrate electrode, this wire surface is modified with zinc oxide nano-particle, as electron transfer layer; One light-emitting polymer layer, is stained with the wire surface being coated in zinc oxide nano-particle and modifying; One transparency electrode, is made up of to be coaxially wrapped in the wire substrate of being stained with and being coated with light-emitting polymer layer many walls orientation carbon nanotube film.Shown in its structural representation Fig. 1.
Because many walls orientation carbon nanotube film has the good transparency and conductivity, as transparency electrode, the efficiency of the luminescence of fibrous electrochemical luminescence battery is improved greatly, and cost reduce greatly.
The invention allows for the preparation method of fibrous electrochemical luminescence battery, concrete steps are as follows:
(1) transparent electrode material is prepared: can spin on carbon nano pipe array at many walls and pull out many walls orientation carbon nanotube film;
(2) prepare fibrous metal silk substrate: wire is stained with painting burnett's solution, then anneals, annealing temperature is 300-600 degree Celsius, and annealing time is 0.5-2 hour, forms zinc oxide nano-particle layer in wire surface; This step repeatedly, makes zinc oxide nano-particle layer have suitable thickness, general thickness 20-100 nanometer, thus obtains the wire that zinc oxide nano-particle modifies as electron transfer layer; Described wire is as steel wire, titanium silk or aluminium wire etc.;
(3) then, the wire surface of modifying at zinc oxide nano-particle is stained with painting one deck light-emitting polymer layer, and places 1-10 hour in vacuum environment; Many walls orientation carbon nanotube film is wound around uniformly in the above as transparency electrode, obtains complete wire luminescent device;
(4) last, the fibrous electrochemical luminescence battery obtained is adopted under the inert gas environment of drying the good macromolecular material encapsulation of sealing.
In the present invention, described light emitting polymer layer material can be the different colours such as polyfluorene or SuperYellow light emitting polymer.
Here prepares the concrete operation step of fibrous electrochemical luminescence battery:
First, forming zinc oxide nano-particle layer by being stained with painting method on wire (as stainless steel wire) surface, then calcining 30 minutes under 300 degrees Celsius in tube furnace and annealing, treating that temperature drops to room temperature and takes out later.This process is repeated 3 times and form certain thickness zinc oxide nano-particle layer as electron transfer layer in wire surface, put into the glove box being full of argon gas; In the glove box being full of argon gas, the stainless steel wire that zinc oxide nano-particle is modified is used for making fibrous electrochemical luminescence battery.By being stained with a kind of derivative PF-B(20-60 mg/mL being coated with luminous polyfluorene), the tetrahydrofuran solution of ethoxylated trimethylolpropane triacrylate and trifluoromethyl sulfonic acid lithium, then vacuumizes one hour; Many walls orientation carbon nanotube film is wrapped in above wire uniformly, the fibrous electrochemical luminescence battery that final formation is complete.Finally, adopt encapsulating material to be encapsulated in the inert gas environment of drying by device, obtain complete fibrous polymer light emitting electrochemical cell.
The carbon nano pipe array used in described orientation carbon nanotube film adopts routine techniques preparation, and concrete steps are:
The catalyst structure of synthesizing carbon nanotubes array is Si/SiO
2/ Al
2o
3/ Fe, wherein, SiO
2thickness is 300-1000 μm, Al
2o
3thickness is 1-30 nm, Fe thickness is 0.5-1.5 nm, Al
2o
3be positioned at the centre of silicon chip and Fe, as resilient coating, Fe is as catalyst, and they deposit the film of one deck nano thickness respectively by electron beam evaporation deposition instrument on silicon chip; Adopt chemical vapour deposition technique, do carbon source with ethene, using argon gas and hydrogen as carrier gas, synthesize height-oriented carbon nano pipe array having on oxide layer Si substrate; Wherein ethene flow is 190-290 sccm, and argon flow amount is 400-620 sccm, and hydrogen flowing quantity is 20-48 sccm, grows 5-20 min in tube furnace.
Fibrous electrochemical luminescence battery prepared by the present invention, effectively can realize 360 degree of luminescences, and has well flexible and woven performance.Coaxial configuration has obviously advantage for the luminescence of device.For luminescent device, in radial directions similar in appearance to plane luminescent device, greatly reduce contact resistance, coaxial configuration has high contact area, is conducive to quick transmission and the transfer of electronics; Adopt multi-wall carbon nano-tube film as transparency electrode simultaneously, improve the luminous efficiency of device greatly, there is vast potential for future development.Multi-wall carbon nano-tube film is that many walls by being synthesized by chemical vapour deposition technique can spin carbon nano pipe array and carry out [21-23] that dry spinning obtains.The mechanism of electrochemical luminescence battery is subject to enough voltage when device two ends, and chemical doping occurs at electroluminescence conjugated polymer two ends, near one end of negative electrode, N-type doping occurring, and near one end of anode, the doping of P type occurring.Due to doping, polymeric layer has higher conductivity.Form PIN junction, be conducive to the effective injection at two ends of electronics and hole, there is compound in final electronics and hole, produces light.In future, fibrous electrochemical luminescence battery will have vast potential for future development at photoelectron fabric arts.The zinc oxide precursor liquid solution that the present invention adopts in an experiment is the Zn (CH of 1.46 g
3cOO)
22H
2the NH of O and 0.2 mL
2cH
2cH
2oH is dissolved in 25 mL CH
3oCH
2cH
2in OH, and stir 30 minutes under 60 degree of conditions.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of fibrous electrochemical luminescence battery, and wire and many walls orientation carbon nanotube film are respectively as the two poles of the earth of fibrous electrochemical luminescence battery.
Fig. 2 has carried out SEM sign to fibrous electrochemical luminescence battery each several part.Wherein, a is wire low power SEM picture.B is that wire surface is stained with the SEM picture after being coated with zinc oxide nano-particle.C and d is stained with to be coated with top view after polymer light-emitting layer and sectional view.E and f is low power after uniform winding orientation carbon nanotube film and high power SEM picture.
Fig. 3 is the voltage-to-current-luminance test curve of fibrous electrochemical luminescence battery.
Fig. 4 is the schematic diagram being wound around orientation carbon nanotube film.
Fig. 5 is the different angles luminescent properties test of fibrous electrochemical luminescence battery.
Fig. 6 is the bending property test of fibrous electrochemical luminescence battery.
Fig. 7 is woven performance and the luminous controllability sign of device.
Fig. 8 is the low power SEM stereoscan photograph that can spin carbon nano pipe array.
Fig. 9 is the high power SEM stereoscan photograph that can spin carbon nano pipe array.
Figure 10 is the pictorial diagram of fibrous electrochemical luminescence battery.
Embodiment
1. prepare transparency electrode, can spin on carbon nano pipe array at many walls and pull out many walls orientation carbon nanotube film.
2. prepare fibrous metal substrate, the wire after cleaning is stained with painting burnett's solution and is annealed at its surface formation zinc oxide nano-particle layer.This step is repeatedly had certain thickness zinc oxide nano-particle layer uniformly, thus is obtained the wire that zinc oxide nano-particle modifies as electron transfer layer.
3. be then stained with painting one deck light-emitting polymer layer by being stained with painting method in the wire surface that zinc oxide nano-particle is modified, this layer is by the copolymer of polyfluorene, ionic conductivity solution and ion component trifluoromethyl sulfonic acid lithium are dissolved in (mass ratio is 20:10:1) in tetrahydrofuran solvent, and place 1 hour in vacuum environment.Many walls orientation carbon nanotube film is wound around uniformly in the above as transparency electrode, obtains complete wire luminescent device.
4. the last good macromolecular material of sealing that adopted under the inert gas environment of drying by the fibrous electrochemical luminescence battery obtained encapsulates.
Threadiness electrochemical luminescence battery structure is characterized by ESEM (Hitachi FE-SEM S-4800 operated at 1 kV).Current-voltage-brightness test curve adopts Keithley 2400 source table and Photoresearch PR-650.Orientation carbon nanotube film transmitance is measured by Shimadzu UV-2550 spectrophotometer.
list of references
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Adv. Mater. 19, 365-370 (2007).
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3. Pei, Q., Yu, G., Zhang, C., Yang, Y. & Heeger, A.J. Polymer Light-Emitting Electrochemical Cells.
Science 269, 1086-1088 (1995).
4. Liang, J., Li, L., Niu, X., Yu, Z. & Pei, Q. Elastomeric polymer light-emitting devices and displays.
Nature Photon. 7, 817-824 (2013).
5. Shao, Y., Gong, X., Heeger, A.J., Liu, M. & Jen, A.K.Y. Long-Lifetime Polymer Light-Emitting Electrochemical Cells Fabricated with Crosslinked Hole-Transport Layers.
Adv. Mater. 21, 1972-1975 (2009).
6. Li, L. et al. Efficient Flexible Phosphorescent Polymer Light-Emitting Diodes Based on Silver Nanowire-Polymer Composite Electrode.
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7. Kuik, M. et al. 25th Anniversary Article: Charge Transport and Recombination in Polymer Light-Emitting Diodes.
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8. H?fle, S., Schienle, A., Bruns, M., Lemmer, U. & Colsmann, A. Enhanced Electron Injection into Inverted Polymer Light-Emitting Diodes by Combined Solution-Processed Zinc Oxide/Polyethylenimine Interlayers.
Adv. Mater. 26, 2750-2754 (2014).
9. Ying, L., Ho, C.-L., Wu, H., Cao, Y. & Wong, W.-Y. White Polymer Light-Emitting Devices for Solid-State Lighting: Materials, Devices, and Recent Progress.
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10. Matyba, P., Yamaguchi, H., Chhowalla, M., Robinson, N.D. & Edman, L. Flexible and Metal-Free Light-Emitting Electrochemical Cells Based on Graphene and PEDOT-PSS as the Electrode Materials.
ACS Nano 5, 574-580 (2010).
11. Reineke, S. et al. White organic light-emitting diodes with fluorescent tube efficiency.
Nature 459, 234-238 (2009).
12. Uoyama, H., Goushi, K., Shizu, K., Nomura, H. & Adachi, C. Highly efficient organic light-emitting diodes from delayed fluorescence.
Nature 492, 234-238 (2012).
13. Groves, C. Organic light-emitting diodes: Bright design.
Nature Mater. 12, 597-598 (2013).
14. Sun, Y. & Forrest, S.R. Enhanced light out-coupling of organic light-emitting devices using embedded low-index grids.
Nature Photon. 2, 483-487 (2008).
15. Han, T.-H. et al. Extremely efficient flexible organic light-emitting diodes with modified graphene anode.
Nature Photon. 6, 105-110 (2012).
16. White, M.S. et al. Ultrathin, highly flexible and stretchable PLEDs.
Nature Photon. 7, 811-816 (2013).
17. Wu, H.B. et al. Efficient Single Active Layer Electrophosphorescent White Polymer Light-Emitting Diodes.
Adv. Mater. 20, 696-702 (2008).
18. Kabra, D., Lu, L.P., Song, M.H., Snaith, H.J. & Friend, R.H. Efficient Single-Layer Polymer Light-Emitting Diodes.
Adv. Mater. 22, 3194-3198 (2010).
19. Yook, K.S. & Lee, J.Y. Small Molecule Host Materials for Solution Processed Phosphorescent Organic Light-Emitting Diodes.
Adv. Mater. 26, 4218-4233 (2014).
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Claims (4)
1. a fibrous electrochemical luminescence battery, is characterized in that comprising:
One wire, as fibrous substrate electrode, this wire surface is modified with zinc oxide nano-particle, as electron transfer layer;
One light-emitting polymer layer, is stained with the wire surface being coated in zinc oxide nano-particle and modifying;
One transparency electrode, is made up of to be coaxially wrapped in the wire substrate of being stained with and being coated with light-emitting polymer layer many walls orientation carbon nanotube film.
2. the preparation method of fibrous electrochemical luminescence battery as claimed in claim 1, is characterized in that concrete steps are:
(1) can spin on carbon nano pipe array at many walls and pull out many walls orientation carbon nanotube film;
(2) prepare fibrous metal silk substrate: wire is stained with painting burnett's solution, then anneals, annealing temperature is 300-600 degree Celsius, and annealing time is 0.5-2 hour, forms zinc oxide nano-particle layer in wire surface; This step repeatedly, makes zinc oxide nano-particle layer have suitable thickness, thus obtains the wire that zinc oxide nano-particle modifies as electron transfer layer;
(3) then, the wire surface of modifying at zinc oxide nano-particle is stained with painting one light-emitting polymer layer, and places 1-10 hour in vacuum environment; Many walls orientation carbon nanotube film is wound around uniformly in the above as transparency electrode, obtains complete wire luminescent device;
(4) last, the fibrous electrochemical luminescence battery obtained is adopted under the inert gas environment of drying the good macromolecular material encapsulation of sealing.
3. the preparation method of fibrous electrochemical luminescence battery according to claim 2, is characterized in that described light emitting polymer layer material is: the different colours such as polyfluorene or SuperYellow light emitting polymer.
4. the preparation method of fibrous electrochemical luminescence battery according to claim 3, is characterized in that the preparation process of described array of multi-walled carbon nanotubes is:
Employing structure is Si/SiO
2/ Al
2o
3the catalyst of/Fe, wherein, SiO
2thickness is 300-1000 μm, Al
2o
3thickness is 1-30 nm, Fe thickness is 0.5-1.5 nm, Al
2o
3be positioned at the centre of silicon chip and Fe, as resilient coating, Fe is as catalyst, and they deposit the film of one deck nano thickness respectively by electron beam evaporation deposition instrument on silicon chip; Adopt chemical vapour deposition technique, do carbon source with ethene, using argon gas and hydrogen as carrier gas, synthesize height-oriented carbon nano pipe array having on oxide layer Si substrate; Wherein ethene flow is 190-290 sccm, and argon flow amount is 400-620 sccm, and hydrogen flowing quantity is 20-48 sccm, grows 5-20 min in tube furnace.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105047999A (en) * | 2015-07-31 | 2015-11-11 | 复旦大学 | Fibrous hybridization energy storage device with high-energy density and high power density, and preparation method thereof |
| CN105244565A (en) * | 2015-10-26 | 2016-01-13 | 复旦大学 | Flexible tensible chargable linear zinc air cell and preparation method thereof |
| CN107564730A (en) * | 2017-07-06 | 2018-01-09 | 复旦大学 | A kind of fluorescent fiber shape ultracapacitor fiber and preparation method thereof |
| CN107680828A (en) * | 2017-09-18 | 2018-02-09 | 西南交通大学 | A kind of stretchable ultracapacitor using stainless steel spring as substrate |
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| CN101485008A (en) * | 2006-05-01 | 2009-07-15 | 维克森林大学 | Organic optoelectronic devices and applications thereof |
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| WO2013113349A1 (en) * | 2012-01-30 | 2013-08-08 | Merck Patent Gmbh | Nanocrystals on fibers |
| CN103400889A (en) * | 2013-07-02 | 2013-11-20 | 复旦大学 | All-solid-state fibrous coaxial polymer solar cell and super capacitor integrated device and preparation method thereof |
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| CN101019248A (en) * | 2004-07-16 | 2007-08-15 | 普林斯顿大学理事会 | Organic devices having a fiber structure |
| CN101485008A (en) * | 2006-05-01 | 2009-07-15 | 维克森林大学 | Organic optoelectronic devices and applications thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105047999A (en) * | 2015-07-31 | 2015-11-11 | 复旦大学 | Fibrous hybridization energy storage device with high-energy density and high power density, and preparation method thereof |
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| CN105244565A (en) * | 2015-10-26 | 2016-01-13 | 复旦大学 | Flexible tensible chargable linear zinc air cell and preparation method thereof |
| CN105244565B (en) * | 2015-10-26 | 2018-06-08 | 复旦大学 | A kind of chargeable linear zinc-air battery of flexible stretching and preparation method thereof |
| CN107564730A (en) * | 2017-07-06 | 2018-01-09 | 复旦大学 | A kind of fluorescent fiber shape ultracapacitor fiber and preparation method thereof |
| CN107680828A (en) * | 2017-09-18 | 2018-02-09 | 西南交通大学 | A kind of stretchable ultracapacitor using stainless steel spring as substrate |
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Address after: 264006 Heilongjiang Road, Yantai economic and Technological Development Zone, Shandong 10 Patentee after: Taihe New Material Group Co.,Ltd. Address before: 264006 Heilongjiang Road, Yantai economic and Technological Development Zone, Shandong 10 Patentee before: YANTAI TAYHO ADVANCED MATERIALS Co.,Ltd. |